CN115142120A - Sapphire electrode protective sleeve and preparation method thereof - Google Patents
Sapphire electrode protective sleeve and preparation method thereof Download PDFInfo
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- CN115142120A CN115142120A CN202210873456.3A CN202210873456A CN115142120A CN 115142120 A CN115142120 A CN 115142120A CN 202210873456 A CN202210873456 A CN 202210873456A CN 115142120 A CN115142120 A CN 115142120A
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- sapphire
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- 229910052594 sapphire Inorganic materials 0.000 title claims abstract description 80
- 239000010980 sapphire Substances 0.000 title claims abstract description 80
- 230000001681 protective effect Effects 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000013078 crystal Substances 0.000 claims abstract description 65
- 238000000034 method Methods 0.000 claims abstract description 18
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 43
- 239000000463 material Substances 0.000 claims description 23
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 21
- 238000001816 cooling Methods 0.000 claims description 15
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 7
- 229910052802 copper Inorganic materials 0.000 claims description 7
- 239000010949 copper Substances 0.000 claims description 7
- 238000000137 annealing Methods 0.000 claims description 6
- 239000000725 suspension Substances 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 229910000831 Steel Inorganic materials 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 239000010959 steel Substances 0.000 claims description 4
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 4
- 229910052721 tungsten Inorganic materials 0.000 claims description 4
- 239000010937 tungsten Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims 1
- 230000010354 integration Effects 0.000 claims 1
- 150000002500 ions Chemical class 0.000 abstract description 8
- 238000009826 distribution Methods 0.000 abstract description 4
- 239000000155 melt Substances 0.000 abstract description 4
- 238000005204 segregation Methods 0.000 abstract description 4
- 229910010293 ceramic material Inorganic materials 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000000126 substance Substances 0.000 description 4
- 239000010453 quartz Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000306 component Substances 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/20—Aluminium oxides
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a sapphire electrode protective sleeve and a preparation method thereof. The preparation method is prepared by an EFG guide die process, and the die is used for one-time forming, so the inner diameter of the die can be freely designed, and the melt in a capillary tube of the die has very high convection. In the preparation method of the sapphire electrode protective sleeve, the segregation coefficient of doped ions is generally close to 1, and the upper and lower ion distribution consistency of crystals is good.
Description
Technical Field
The invention relates to the technical field of component equipment, in particular to a sapphire electrode protective sleeve and a preparation method thereof.
Background
The field of high-temperature material preparation depends on high-temperature equipment, and due to the particularity of the process, the high-temperature material preparation has the characteristics of long working period and high material cost, and the stability and repeatability of the high-temperature equipment are in urgent need. The heating electrode is regarded as one of the core components of the high-temperature equipment, and is paid much attention, in order to avoid abnormal phenomena (such as power supply tripping, electrode or heating element damage, water leakage and the like) such as ignition, overcurrent and the like, an electrode protective sleeve is often additionally arranged on the outer wall of the electrode to protect the electrode.
The traditional electrode sheath material is mostly quartz material, alumina ceramic material and the like. Although the chemical properties of the quartz and the protective sleeve are stable at normal temperature, the softening point of the quartz is low (1200 ℃), the use temperature range is limited, the phenomenon of simple substance silicon precipitation can occur at about 1500 ℃, the simple substance silicon often has the effect of electric conductivity and can damage the insulation effect of the protective sleeve, the traditional alumina ceramic has the working temperature of about 1600 ℃, and is very easy to be carbonized under the carbon atmosphere, so that the material is deoxidized, the phenomenon of simple substance aluminum precipitation occurs, the mechanical strength of the insulation property and the protective sleeve is influenced, and the material is cracked.
The alumina ceramic material has unsatisfactory tightness, and is easily polluted by impurities in the use environment, so that the insulativity of the alumina ceramic material is damaged; meanwhile, the ceramic material has poor thermal shock resistance, and is cracked when being subjected to thermal stress shock in the repeated use process at high temperature, so that the ceramic material becomes a vulnerable part and increases the use cost.
Disclosure of Invention
The invention aims to provide a sapphire electrode protective sleeve and a preparation method thereof, wherein a mould is used for one-step forming, so the inner diameter of the sapphire electrode protective sleeve can be freely designed, the convection of a melt in a capillary tube of the mould is weak, the segregation coefficient of doped ions in a crystal is generally close to 1, and the distribution consistency of upper and lower ions of the crystal is good.
In order to achieve the above purpose, the invention provides the following technical scheme:
the invention provides a sapphire electrode protective sleeve which comprises a sapphire electrode protective sleeve, wherein a sapphire gasket is fixedly connected to the bottom of the sapphire electrode protective sleeve, a water-cooling furnace bottom plate is fixedly connected to the bottom of the sapphire electrode protective sleeve, an insulating sealing ring is fixedly connected to the center inside the water-cooling furnace bottom plate, and the sapphire electrode protective sleeve and the sapphire gasket are integrated.
The sapphire electrode protection sleeve and the sapphire gasket comprise the following preparation steps:
step S110: manufacturing a growth mould A according to the height of the sapphire electrode protection sleeve and the sapphire gasket being 50-300 mm and the inner diameter being 10-150 mm, and arranging a material supply seam with the aperture being 2-3 mm at the bottom of the growth mould A;
step S120: the growth mould A is arranged above the center of the crucible in a suspension mode;
step S130: placing high-purity alumina crushed crystal grains in a crucible, vacuumizing the crucible, and filling protective atmosphere;
step S140: heating the crucible to 2100-2200 ℃ to heat and melt the high-purity alumina crushed grains to obtain an alumina melt A;
step S150: after the high-purity aluminum oxide crushed grains are completely melted, the crucible is lifted to enable the growth mold A to be immersed into the aluminum oxide melt A, and the aluminum oxide melt A is lifted to the surface of the growth mold A through a feeding slit arranged on the growth mold A by siphoning;
step S160: descending a seed crystal rod to enable two ends of a seed crystal to contact with material supply seams on two sides of a growth mould A, then starting to lift and shoulder until an alumina melt grows into a complete circular ring shouldered crystal, and then starting to wait for a radial growth process;
step S170: and after the growth of the ring shouldered crystal is finished, the seed rod is quickly pulled to be separated from the surface of the growth mold A, the crucible is lowered to separate the excess material in the crucible from the growth mold A to form a crystal blank, and the crystal blank is annealed to obtain the final integrated finished product of the sapphire electrode protective sleeve and the sapphire gasket.
Compared with the prior art, in the preparation method of the sapphire electrode protective sleeve, after high-purity aluminum oxide crushed grains are completely melted, the crucible is lifted to immerse the growth mold A into the aluminum oxide melt A, the aluminum oxide melt A is lifted to the surface of the growth mold A through the feeding seam arranged on the growth mold A through the siphoning effect, the seed crystal rod is lowered to enable two ends of the seed crystal to be in contact with the feeding seams on two sides of the growth mold A, then the pulling and shouldering are started until the aluminum oxide melt grows into a complete circular shouldered crystal, then the diameter growth process is started to wait, the sapphire electrode protective sleeve is a sapphire single crystal tube and can be prepared through an EFG (edge melt diffusion) guide mold process, the mold is used for one-time forming, the inner diameter of the sapphire electrode protective sleeve can be freely designed, the convection of the melt in a capillary tube of the mold is weak, the segregation coefficient of doped ions in the crystal is generally close to 1, and the upper and lower ion distribution of the crystal is good.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is a schematic view showing an installation state of a sapphire electrode protection sleeve, a sapphire gasket and a high-temperature graphite electrode according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of the growth of a sapphire crystal in an embodiment of the present invention.
Wherein, 1, sapphire electrode protective sleeve; 2. a sapphire spacer; 3. a high temperature graphite electrode; 4. water-cooling the furnace bottom plate; 5. an insulating seal ring; 6. water-cooling the copper electrode.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The embodiment of the invention is shown in figure 1, and provides a sapphire electrode protection sleeve which comprises a sapphire electrode protection sleeve 1, wherein the bottom of the sapphire electrode protection sleeve 1 is fixedly connected with a sapphire gasket 2, the bottom of the sapphire electrode protection sleeve 1 is fixedly connected with a water-cooling furnace bottom plate 4, the center inside the water-cooling furnace bottom plate 4 is fixedly connected with an insulating sealing ring 5, and the sapphire electrode protection sleeve 1 and the sapphire gasket 2 are arranged into an integrated body.
Insulating seal 5 inside centers of circle is provided with water-cooling copper electrode 6, and 6 upper portions of water-cooling copper electrode extend to sapphire electrode protective case 1 inside, and 6 tops of water-cooling copper electrode are provided with high temperature graphite electrode 3, and sapphire electrode protective case can handle through the form of washing or mechanical polishing, uses repeatedly, and then reduces use cost.
The embodiment of the invention provides a sapphire electrode protective sleeve, wherein the sapphire electrode protective sleeve 1 and a sapphire gasket 2 comprise the following preparation steps:
step S110: manufacturing a growth mould A according to the height of the sapphire electrode protection sleeve 1 and the sapphire gasket 2 being 150 mm and the body size of the inner diameter being 50 mm, and arranging a feeding seam with the aperture being 2 mm at the bottom of the growth mould A;
step S120: the growth mould A is arranged above the center of the crucible in a suspension mode;
step S130: placing the high-purity alumina crushed crystal grains in a crucible, wherein the alumina purity of the high-purity alumina crushed crystal grains is 95%, vacuumizing the crucible, and then filling a protective atmosphere, wherein the protective atmosphere is high-purity argon with the content of 90%;
step S140: heating the crucible to 2100 ℃ to heat and melt the high-purity alumina crushed grains to obtain an alumina melt A;
step S150: after the high-purity alumina crushed grains are completely melted, the crucible is lifted to enable the growth mould A to be immersed into the alumina melt A, and the alumina melt A is lifted to the surface of the growth mould A through a feeding seam arranged on the growth mould A by a siphoning effect;
step S160: descending a seed crystal rod to enable two ends of a seed crystal to contact with material supply seams on two sides of a growth mould A, then starting to lift and shoulder, setting the lifting speed to be 10 mm per hour until an alumina melt grows into a complete circular shoulder crystal, and then starting to wait for a radial growth process;
step S170: after the growth of the ring shouldered crystal is finished, the seed rod is quickly pulled to be separated from the surface of the growth mold A, the crucible is lowered to separate the excess material in the crucible from the growth mold A to form a crystal blank, after the crystal blank is annealed, the annealing and cooling time of the crystal blank is ensured to be more than 6 hours, and finally an integrated finished product of the sapphire electrode protective sleeve 1 and the sapphire gasket 2 is obtained.
Compared with the prior art, in the preparation method of the sapphire electrode protective sleeve, after high-purity aluminum oxide crushed grains are completely melted, the crucible is lifted to immerse the growth mold A into the aluminum oxide melt A, the aluminum oxide melt A is lifted to the surface of the growth mold A through the feeding seam arranged on the growth mold A through the siphoning effect, the seed crystal rod is lowered to enable two ends of the seed crystal to be in contact with the feeding seams on two sides of the growth mold A, then the pulling and shouldering are started until the aluminum oxide melt grows into a complete circular shouldered crystal, then the diameter growth process is started to wait, the sapphire electrode protective sleeve is a sapphire single crystal tube and can be prepared through an EFG (edge melt diffusion) guide mold process, the mold is used for one-time forming, the inner diameter of the sapphire electrode protective sleeve can be freely designed, the convection of the melt in a capillary tube of the mold is weak, the segregation coefficient of doped ions in the crystal is generally close to 1, and the upper and lower ion distribution of the crystal is good.
The following describes each step in the preparation method of the sapphire electrode protective sleeve provided by the embodiment of the invention in detail.
As shown in fig. 2, in step S110: according to the height 150 mm of the sapphire electrode protection sleeve 1 and the sapphire gasket 2 and the size of the body with the inner diameter of 50 mm, a growth mold A is manufactured, and a feeding seam with the aperture of 2 mm is arranged at the bottom of the growth mold A.
In step S120: the growth mould A is arranged above the center of the crucible in a suspension mode;
wherein the crucible is made of tungsten material, and can also be made of steel material.
In step S130: placing the high-purity alumina crushed grains in a crucible, wherein the alumina purity of the high-purity alumina crushed grains is 95%, vacuumizing the crucible, and filling protective atmosphere.
In step S140: heating the crucible to 2100 ℃ to heat and melt the high-purity alumina crushed grains to obtain alumina melt A.
In step S150: after the high-purity aluminum oxide crushed grains are completely melted, the crucible is lifted to enable the growth mold A to be immersed into the aluminum oxide melt A, and the aluminum oxide melt A is lifted to the surface of the growth mold A through a feeding slit arranged on the growth mold A under the siphoning action.
In step S160: and (3) descending the seed crystal rod to enable two ends of the seed crystal to be in contact with the material supply seams on two sides of the growth mould A, then starting to lift and shouldering, setting the lifting speed to be 10 mm per hour until the alumina melt grows into a complete circular ring shouldered crystal, and then starting to wait for the radial growth process.
In step S170: after the growth of the ring shouldered crystal is finished, the seed rod is quickly pulled to be separated from the surface of the growth mold A, the crucible is lowered to separate the excess material in the crucible from the growth mold A to form a crystal blank, after the crystal blank is annealed, the annealing and cooling time of the crystal blank is ensured to be more than 6 hours, and finally an integrated finished product of the sapphire electrode protective sleeve 1 and the sapphire gasket 2 is obtained.
In order to explain the preparation method of the sapphire electrode protective sleeve provided by the embodiment of the invention in detail, the following gives a detailed description in combination with the embodiment.
Example one
The embodiment provides a preparation method of a sapphire electrode protective sleeve, which comprises the following steps:
step S110: according to the height 150 mm of the sapphire electrode protection sleeve 1 and the sapphire gasket 2 and the size of the body with the inner diameter of 50 mm, a growth mold A is manufactured, and a feeding seam with the aperture of 2 mm is arranged at the bottom of the growth mold A.
Step S120: the growth mould A is arranged above the center of the crucible in a suspension mode, and the crucible is made of tungsten or steel.
Step S130: placing the high-purity alumina crushed crystal grains in a crucible, wherein the alumina purity of the high-purity alumina crushed crystal grains is 95%, vacuumizing the crucible, and then filling a protective atmosphere, wherein the protective atmosphere is high-purity argon with the content of 90%.
Step S140: heating the crucible to 2100 ℃ to heat and melt the high-purity alumina crushed grains to obtain the alumina melt A.
Step S150: after the high-purity alumina crushed grains are completely melted, the crucible is lifted to enable the growth mould A to be immersed into the alumina melt A, and the alumina melt A is lifted to the surface of the growth mould A through a feeding slit arranged on the growth mould A under the siphonage action.
Step S160: and (3) descending the seed crystal rod to enable two ends of the seed crystal to contact with the material supply seams on two sides of the growth mould A, then starting to pull and shoulder, setting the pulling speed to be 10 mm per hour until the aluminum oxide melt grows into a complete circular ring shouldered crystal, and then starting to wait for the growth process.
Step S170: after the growth of the ring shouldered crystal is finished, the seed rod is quickly pulled to be separated from the surface of the growth mold A, the crucible is lowered to separate the excess material in the crucible from the growth mold A to form a crystal blank, after the crystal blank is annealed, the annealing and cooling time of the crystal blank is ensured to be more than 6 hours, and finally an integrated finished product of the sapphire electrode protective sleeve 1 and the sapphire gasket 2 is obtained.
Example two
Step S110: according to the height 150 mm of the sapphire electrode protection sleeve 1 and the sapphire gasket 2 and the size of the body with the inner diameter of 50 mm, a growth mold A is manufactured, and a feeding seam with the aperture of 2 mm is arranged at the bottom of the growth mold A.
Step S120: the growth mould A is arranged above the center of the crucible in a suspension mode, and the crucible is made of tungsten or steel.
Step S130: placing the high-purity alumina crushed crystal grains in a crucible, wherein the alumina purity of the high-purity alumina crushed crystal grains is 95%, vacuumizing the crucible, and then filling a protective atmosphere, wherein the protective atmosphere is high-purity argon with the content of 90%.
Step S140: heating the crucible to 2100 ℃ to heat and melt the high-purity alumina crushed grains to obtain the alumina melt A.
Step S150: after the high-purity aluminum oxide crushed grains are completely melted, the crucible is lifted to enable the growth mold A to be immersed into the aluminum oxide melt A, and the aluminum oxide melt A is lifted to the surface of the growth mold A through a feeding slit arranged on the growth mold A through siphoning.
Step S160: and (3) descending the seed crystal rod to enable two ends of the seed crystal to be in contact with the material supply seams on two sides of the growth mould A, then starting to lift and shouldering, setting the lifting speed to be 10 mm per hour until the alumina melt grows into a complete circular ring shouldered crystal, and then starting to wait for the radial growth process.
Step S170: after the growth of the ring shouldered crystal is finished, the seed rod is quickly pulled to be separated from the surface of the growth mold A, the crucible is lowered to separate the excess material in the crucible from the growth mold A to form a crystal blank, after the crystal blank is annealed, the annealing and cooling time of the crystal blank is ensured to be more than 6 hours, and finally an integrated finished product of the sapphire electrode protective sleeve 1 and the sapphire gasket 2 is obtained.
In the foregoing description of embodiments, the particular features, structures, materials, or characteristics may be combined in any suitable manner in any one or more embodiments or examples.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily think of the changes or substitutions within the technical scope of the present invention, and shall cover the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (8)
1. The utility model provides a sapphire electrode protective sheath, includes sapphire electrode protective sleeve (1), its characterized in that: sapphire electrode protective case (1) bottom fixed connection sapphire gasket (2), sapphire electrode protective case (1) bottom fixed connection water-cooling furnace bottom plate (4), insulating sealing washer (5) of inside center fixed connection of water-cooling furnace bottom plate (4), sapphire electrode protective case (1) and sapphire gasket (2) set up to the integration shape.
2. The sapphire electrode protective sleeve according to claim 1, wherein a water-cooled copper electrode (6) is arranged in the center of the inside of the insulating sealing ring (5), the upper part of the water-cooled copper electrode (6) extends into the inside of the sapphire electrode protective sleeve (1), and a high-temperature graphite electrode (3) is arranged at the top end of the water-cooled copper electrode (6).
3. The sapphire electrode sheath of claim 1, wherein: the sapphire electrode protection sleeve (1) and the sapphire gasket (2) comprise the following preparation steps:
step S110: manufacturing a growth mould A according to the height of the sapphire electrode protective sleeve (1) and the sapphire gasket (2) being 50-300 mm and the body size of the inner diameter being 10-150 mm, and arranging a feeding seam with the aperture being 2-3 mm at the bottom of the growth mould A;
step S120: the growth mould A is arranged above the center of the crucible in a suspension mode;
step S130: placing the high-purity alumina crushed crystal grains in a crucible, vacuumizing the crucible, and filling protective atmosphere;
step S140: heating the crucible to 2100-2200 ℃ to heat and melt the high-purity alumina crushed grains to obtain an alumina melt A;
step S150: after the high-purity aluminum oxide crushed grains are completely melted, the crucible is lifted to enable the growth mold A to be immersed into the aluminum oxide melt A, and the aluminum oxide melt A is lifted to the surface of the growth mold A through a feeding slit arranged on the growth mold A by siphoning;
step S160: descending a seed crystal rod to enable two ends of a seed crystal to contact with material supply seams on two sides of a growth mould A, then starting to lift and shoulder until an alumina melt grows into a complete circular ring shouldered crystal, and then starting to wait for a radial growth process;
step S170: after the growth of the ring shouldered crystal is finished, the seed rod is quickly pulled to be separated from the surface of the growth mold A, the crucible is lowered to separate the excess materials in the crucible from the growth mold A, a crystal blank is formed, and the final integrated finished product of the sapphire electrode protective sleeve (1) and the sapphire gasket (2) is obtained after annealing operation is carried out on the crystal blank.
4. The method as claimed in claim 3, wherein the crucible is made of tungsten or steel in step S1320.
5. The method of claim 3, wherein the alumina purity of the high purity alumina crushed grains is 93-98% in step S130.
6. The method of claim 3, wherein the protective atmosphere is high purity argon gas at a content of 90-95% in step S130.
7. The method of claim 3, wherein the pull rate is set to 10 to 20 mm per hour in step S160.
8. The method of claim 3, wherein in step S170, the time for annealing the crystal blank is ensured to be longer than 6 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210873456.3A CN115142120A (en) | 2022-07-21 | 2022-07-21 | Sapphire electrode protective sleeve and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210873456.3A CN115142120A (en) | 2022-07-21 | 2022-07-21 | Sapphire electrode protective sleeve and preparation method thereof |
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| Publication Number | Publication Date |
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| CN115142120A true CN115142120A (en) | 2022-10-04 |
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| CN202210873456.3A Pending CN115142120A (en) | 2022-07-21 | 2022-07-21 | Sapphire electrode protective sleeve and preparation method thereof |
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| Country | Link |
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| CN (1) | CN115142120A (en) |
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- 2022-07-21 CN CN202210873456.3A patent/CN115142120A/en active Pending
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